Process for collecting and utilizing aluminum chloride



Nov. 1, 1927. 1,647,446

E. R. WOLCOTT PROCESS FOR COLLECTING AND UTILIZING ALUMINUM CHLORIDE Filed Sept. '7. 1920 ac a 5 5 l Fig.5.

d; J 37% E IN VEN TOR. [ason M71005 ATTOR EY..

Patented Nov. 1, 1927.

UNITED STATE PATET orr cs.

EDSON a. WOLCOTT, on n05 ANenLns, CALIFORNIA, ASSIGNOR, BY MESNE AssIoN- IrnN'rs, TO THE TEXAS COMPANY, OFINEW YORK, N. Y., A CORPORATION on DELA- WARE.

rnocnss non coLLnc'rINe ANn o'rILIzINe ALUMINUM c 'ILonInn.

Application filed September 7, 1920. Serial No. 408,695.

.Thisinvention relates to the manufacture and utilization of aluminum chloride, particularly as an agent for use in petroleum refining. When used for this purpose, it

5 is essential that the aluminum chloride should be substantially anhydrous and free irom basic salt and it is, therefore, essential that the aluminum chloride should be protected from moisture in any form, since in the presence of moisture anhydrous aluminum chloride rapidly decomposes, forming hydrochloric acid and a hydratedv salt or basic salt, which is ineifective as a catalytic agent for the purpose stated.

The main object of my invention is to provide for protection of the aluminum chloride from contact with moisture, for example, the moisture contained in atmos pheric air, from the time at which it leaves the retort or apparatus in which it is produced to the'time at which it is utilized as a catalytic agent.

The accompanying drawings illustrate, diagrammatically, apparatus suitable for 5 carrying out my invention," and referring thereto: v

Fig. 1 is a vertical section of one form of such an apparatus;'

Fig. 2 is a vertical section of another form thereof; 7

Fig. 3 is a vertical section of another form of apparatus adapted for passing the aluminum chloride in vapor or fume form directly into contact with the petroleum to be treated in the refinin operation;

Fig. 4 is a orizontal section showing another form of such apparatus;

Fig. 5 is a section on line 5-5 in Fig. 4;

Fig. 6 is a section on line 6-6 in Fig. 5.

The. apparatus shown in Fig. 1 comprises a chamber or casing 1, having an inlet pipe or connection 2 commumcating with the outlet of a retort 3 in which aluminum chloride is produced and evolved, said chamber 1 having at its bottom an outlet 4 dischargin into a collecting tank 6. Means are provi ed for spraying into chamber 1 a liquid capable of acting as a protective medium for the aluminum chloride, such liquid being, for example, alcohol, carbon-disulphide, car- 60 bontetrachloride, ethylene-chloride, or equivalent liquid, which is capable either of dissolving aluminum chloride or of covering and submerging the same, so as in either case to substantially prevent access of atmospheric air to the aluminum chloride dissolved or contained therein. For the purpose of bringing the aluminum chloride into efiective contact with this liquid and also for the prupose of enabling the liquid to act as a collecting agent for the aluminum chloride, I prefer to spray the liquid into the chamber 1, for example, by means of a spray nozzle 7 to which the liquid is forced bya pump 8, having an intake pipe 9 extending 55 into the body of liquid 10 into the collecting chamber 6 and having an outlet pipe 11 leading to spray nozzle 7. Chamber 1 is also provided with an outlet pipe 12-for residual gas, which may have a sealing means 45 for preventing entrance of'atmospherie air to the chamber 1. Said sealing means may consist of a film of liquid (such as sulphuric acid. or of oil, for example, petroleum) supplied by pump 46 through pipe 53 to the upper end of a screen 55 in a chamber 56, such liquid running down on the screen to an outlet pipe 57 which returns it to pump ,46. The gases passing from chamber 1 have suflicient power to break through this film of liquid, but said film prevents diffusion of air back to the chamber. The outlet 58 of chamber 56 may be connected to any sultable. means for utilizing residual gas. cooling pipe 59 may be provided for redueing the temperature of the fume before It enters the spray chamber 1, so as avoid overheating of the liquid, which might result in chemical or catalytic actlon.

- The operation of my process as carried I out in the apparatus above described is as follows: i

Aluminum chloride is generated or produced in retort or apparatus 3 in any usual or .suitable manner and the vapor of aluminum chloride, together with any other gases or vapor constituents that ma. be present, passes through thepipe 2 to t e chamber 1 desired, by pump 8 and sired, through a valve 13 into suitable receptacle or container 14. Said; container or receptacle may be provided with a closure means 15 whereby it may be sealed for transportation or storage until it iseventually delivered into the petroleum refining apparatus' If desired, however, the liquid con taining the aluminum chloride'may be piped directly to the point of utilization, for ex- .ample, -to"a petroleum refining retort. In

either case, the anhydrous aluminum chloride is maintained in anhydrous condition until it is introduced into the refining apparatus.

' Instead of spraying the protective liquid into a body of as containing the aluminum chloride, such in of gas maybe passed through a contact 'a sorption tower or chamber, such as indicated at 16 in Fi 2, the gas containing the aluminum chlori e entering at an inlet 17 and passing through checkerwork, or. equivalent means. 22,'and passing preliminary distillation of carboniferous out at an outlet 18, and the protective liquid being sprayed onto the checkerwork 22 from a supply 'ipe 1 9 connected to any suitab le source of t e'protective li uid. As indicated in this figure, the outlet or the liquid containing the aluminum chloride may be provided with a pipe 21 leading to the point where it is to be utilized. p

'Whil' the aluminum chloride may bezproduced' in any suitable manner, I prefer to produce it by subjecting aluminum silicate I V material, such as cla-y'or shale, to the action of chlorine and heat in the presence of carbon, and, for this purpose, the retort 3, indicated in Fig. 1,,may be heated by means of a .furnace 5 and ma be provided with a' supply pipe 20 for c orine. The charge "of cla or other aluminum silicate material, an of carbon produced, :Eor 'example,.by a

material contained in or mixed with the clay,

' is assumed to be substantially free from moisture by reason of the preliminary heating and distillation, so that the product of reaction with the chlorineeutering through 'pipe'3' is substantiallyanhydrous aluminum chloride, which passes through the outlet 2.

inthe form of fume and is collected by spray issuing .t'rom nozzle 7'. The residual gas in conducted'to any suitable means for utilia} ing the same. Aluminum chloride prepared in this manner generally contains more or less ferric chloride from iron com ound present in the clay or shale used,- and y introducing the product in the manner stated into a suitable liquid, for example, either methyl or ethyl alcohol, I efiect a separatlon of the ferric chloride from the aluminumchloride, ferric chloride being-more readily soluble in such liquid, and passing into solution, whereas aluminum chloride is less soluble and remains largely undissolved, and may be separated by decantation or by filthe stated case consists merely'of monoxide, with some chlormeyand maybe tration. Absolute grain alcohol'is not required, as any small amount of water present will only result in production of a corre- 'sponding amount of aluminum hydrate.

The liquid brought-into contact with the anhydrous aluminum chloride may be ca- 4 pableof reaction therewith, and, in such case, the apparatus may be of a type, such as shown in Fig. ,3, adapted to pass the aluminum chloride va or or fume directly from the retort or pro ucer 23 through outlet 25 to. aretort or reaction chamber 24 provided .with an outlet 31, with means 26 for spraying the reacting liquid thereinto, and with means for maintaining said retort 24 at proper temperature for reaction For this purpose the waste gases from the furnace 27, whichserves to heat the aluminum chloride producer or retort 23 may be passed through a casing 28 around the retort or,

reaction chamber 24. The liquid may be circulated by'pump 30, so as to be continuously sprayed through the body of gas and vapor ascendingfin the chamber 24,'thereby washing out the aluminum chloride free from such body of gas or vapor and at the same time giving-maximum contact for reaction between the aluminum chloride and,

the said liquid. The liquid in this case may consist of petroleum or petroleum product from which it isdesired to produce a more volatile product of greater value, and, in

such case", the gases .or vapors passing through outlet 31 of chamber 24 will contain such relatively volatile product, which iscondensed and collected 'in any suitable manner. Retort. 23 may be supplied with chlorine from a pipe 32 and the aluminum chloride may be produced in said retort in fume of aluminum chlorideifiiassing into chamber 24. The liquid sprayed intothe fume inchamber 24 acts as a collecting agent for the aluminum chloride causing the latter to be takerrup by and containedinthe body.

'ofliguid and eventually to react with the liqui collecting liquid.

for example, inefiectingapetroleum refinlngoperation, petroleum is used as the,

. mthe manner above described, the resultmg sulfuric acid. or any suitable oil, for pre-- and 39 (consisting, for example, of brushes having operating handles 42 and 43 working through stufling boxes 44) for brushing or scraping any aluminum chloride which may be deposited on the walls of such piping and forcing it eventually into .the collectionv chamber 34. Said collecting chamber is provided with an outlet 40 for the residual gases and with a filter or screen41 between the inlet pipe 37 and the outlet 40 of the said chamber 34, said screen being preferably above the point of communication of said inlet pipe 37 with the chamber 34, so that the gases ascend in passing from the said inlet pipe to the outlet 40. Under these conditions, I have found that by making the collecting chamber 34 of sufiic-ient dimensions, so as to provide for a very slow upward movement. that the major portion of the aluminum chloride fume may be caused to settle to the lower part of the chamber 34,-so that little, if any, deposit is formed in the filter 41, which, however, acts as a safe-guard against any loss of aluminum. chloride fume.

The material collected in the lower part of the collecting chamber 34 may be removed through outlet openings 48 into receptacles 49 and, if necessary, scraping means 50 maybe provided for scraping the bottom of the chamber 34 to cause the collected material .to fall through the outlet openings 48. I prefer to provide double gates or valves 51 and 52 for the outlets '48 i of the chamber 34, these gates being alternately operated to permit of the discharge of collected material without admitting air'to the chamber 34. Each receptacle 49 may be provided with aclosure means 53 whereby it may be tightly closed-after charging. The outlet 40 of chamber 34 may have a liquid seal containing suit-able liquid, such as venting difiusion of atmospheric air into said chamber. When the liquid is applied to the aluminum chlorideifor the purpose of protecting the same from access of moisture, it is desirable to use a liquid which is non-hygroscopic, so that it will not absorb moisture from the atmosphere.

What I claim is: Y 7

1. The rocess of preparing andmaintaining anhy drous condition, which consists in bringmg the anhydrous ,aluminum chloride into a body ofcprotective liquid undersuch condiiron chloride a non-aqueous rous aluminum chloride in anhy-c tions of temperature as to avoid catalytic decomposition whereby the aluminum chloride is substantially protected from contact with atmospheric air.

2. The process of preparin and maintaining anhydrous aluminum ch oride in anhydrous condition, which consists in introducing aluminum chloride vapors into a body of protective liquid which is inert with respect to the aluminum chloride and is nonhygroscopic, so as to' cover and protect the aluminum chloride from contact with atmospheric air.

.3. The process which consists in roducing a fume of aluminum chloride an spraying a non-hygroscopic li uid into said fume to collect the fume in suc liquid.

4. The process of preparing and maintaining anhydrous aluminum chloride in anhydrous condition, which consists in brin ing the anhydrous aluminum chloride in vaporous form into a body of protective liquid whereby the aluminum chloride issubstantially protected from contact with atmospheric air. a. 1

5. The process which comprises producing anhydrous aluminum chloride in the vaporous state, and spraying said product with a protective liquid to prevent its exposure to atmospheric moisture and to thus maintain the aluminum chloride in anhydrous condition.

6. The process which comprises producing aluminum chloride in the vaporous state, collecting the productstill in anh drous condition by spraying it with a nonygroscopic protective liquid whereby it is kept free from contact with atmospheric moisture.

7. The process which consistsin reducing anhydrous aluminum chloride in t evaporous state in a heated chamber, delivering said product while still in heated and vaporous condition into a contact chamber where it is intimately contacted with a protective liquid, delivering the resulting product into a receiver and preventing the acess of atmosratus during the rocess whereby the aluminum chloride ultimately collected in the receiver is in anhydrous condition.

8. The process which consists in eneratm vapors comprising aluminum chlbride an contactin said vapors with a non-aqueous solvent 0 the aluminum chloride.

9. The process which consists in generatin vapors comprising alummum chlor de an and washing said vapors with fluid having a greater solvent aflinity for the ferric chloride than for the aluminum chloride.

\ :10. The process which consists in ener- "ating vapors comprising aluminum ch oride and iron chloride and washing said vapors v with alcohol.

11. The process which consists 1n genercontaining iron chloride from that contains ing the a1uminun1 chloride.

12. The process that consists in generating Vapors comprlslng alumlnum chloride and contacting said vapors with a non-aqueous liquid so as to absorbthe aluminum chloride therein. 10

In testimony whereof I have hereunto subscribed my name this 26th day of August,

EDSON R. VVOLCOTT. 

